CN114502630A - Resin composition and resin sheet - Google Patents
Resin composition and resin sheet Download PDFInfo
- Publication number
- CN114502630A CN114502630A CN202080068326.1A CN202080068326A CN114502630A CN 114502630 A CN114502630 A CN 114502630A CN 202080068326 A CN202080068326 A CN 202080068326A CN 114502630 A CN114502630 A CN 114502630A
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- China
- Prior art keywords
- resin composition
- resin
- mass
- semi
- examples
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000011342 resin composition Substances 0.000 title claims abstract description 155
- 229920005989 resin Polymers 0.000 title claims abstract description 107
- 239000011347 resin Substances 0.000 title claims abstract description 107
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims abstract description 87
- 229910001701 hydrotalcite Inorganic materials 0.000 claims abstract description 87
- 229960001545 hydrotalcite Drugs 0.000 claims abstract description 87
- 229920005672 polyolefin resin Polymers 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000007789 sealing Methods 0.000 claims description 43
- 239000010410 layer Substances 0.000 description 77
- 239000003795 chemical substances by application Substances 0.000 description 40
- 125000004018 acid anhydride group Chemical group 0.000 description 30
- -1 ethylene, propylene, 1-butene Chemical class 0.000 description 29
- 239000003208 petroleum Substances 0.000 description 29
- 125000003700 epoxy group Chemical group 0.000 description 28
- 239000002966 varnish Substances 0.000 description 28
- 238000010438 heat treatment Methods 0.000 description 21
- 230000004888 barrier function Effects 0.000 description 18
- 229920001577 copolymer Polymers 0.000 description 18
- 150000001875 compounds Chemical class 0.000 description 17
- 239000007788 liquid Substances 0.000 description 17
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 16
- 229910052791 calcium Inorganic materials 0.000 description 16
- 239000011575 calcium Substances 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 16
- 230000006866 deterioration Effects 0.000 description 16
- 229920001083 polybutene Polymers 0.000 description 16
- 229920000139 polyethylene terephthalate Polymers 0.000 description 16
- 239000005020 polyethylene terephthalate Substances 0.000 description 16
- 238000000034 method Methods 0.000 description 15
- 238000001035 drying Methods 0.000 description 14
- 239000011521 glass Substances 0.000 description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 13
- 239000006087 Silane Coupling Agent Substances 0.000 description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 12
- 239000000203 mixture Substances 0.000 description 12
- 229920006255 plastic film Polymers 0.000 description 12
- 239000002985 plastic film Substances 0.000 description 12
- 125000003118 aryl group Chemical group 0.000 description 11
- 239000000126 substance Substances 0.000 description 11
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 11
- 125000002723 alicyclic group Chemical group 0.000 description 10
- 150000001336 alkenes Chemical class 0.000 description 10
- 229910052782 aluminium Inorganic materials 0.000 description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 10
- 238000011156 evaluation Methods 0.000 description 10
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 9
- 239000004014 plasticizer Substances 0.000 description 9
- 230000001681 protective effect Effects 0.000 description 9
- 238000010521 absorption reaction Methods 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 8
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 8
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 8
- 229920005675 propylene-butene random copolymer Polymers 0.000 description 8
- 239000002245 particle Substances 0.000 description 7
- 229920001296 polysiloxane Polymers 0.000 description 7
- 230000002829 reductive effect Effects 0.000 description 7
- 229920006395 saturated elastomer Polymers 0.000 description 7
- 150000003505 terpenes Chemical class 0.000 description 7
- 235000007586 terpenes Nutrition 0.000 description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- MGJKQDOBUOMPEZ-UHFFFAOYSA-N N,N'-dimethylurea Chemical class CNC(=O)NC MGJKQDOBUOMPEZ-UHFFFAOYSA-N 0.000 description 6
- 239000011888 foil Substances 0.000 description 6
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 6
- 229920002799 BoPET Polymers 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 235000014113 dietary fatty acids Nutrition 0.000 description 5
- 239000000194 fatty acid Substances 0.000 description 5
- 229930195729 fatty acid Natural products 0.000 description 5
- 150000004665 fatty acids Chemical class 0.000 description 5
- 239000000945 filler Substances 0.000 description 5
- 238000005984 hydrogenation reaction Methods 0.000 description 5
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 239000000178 monomer Substances 0.000 description 5
- 239000003960 organic solvent Substances 0.000 description 5
- 230000035699 permeability Effects 0.000 description 5
- 229920005673 polypropylene based resin Polymers 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000013032 Hydrocarbon resin Substances 0.000 description 4
- 125000001931 aliphatic group Chemical group 0.000 description 4
- 150000001343 alkyl silanes Chemical class 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 4
- 229920006270 hydrocarbon resin Polymers 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 239000011229 interlayer Substances 0.000 description 4
- 229920013639 polyalphaolefin Polymers 0.000 description 4
- 238000000634 powder X-ray diffraction Methods 0.000 description 4
- 238000000985 reflectance spectrum Methods 0.000 description 4
- 229930195734 saturated hydrocarbon Natural products 0.000 description 4
- 239000000565 sealant Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 229920006132 styrene block copolymer Polymers 0.000 description 4
- 238000004381 surface treatment Methods 0.000 description 4
- 239000012756 surface treatment agent Substances 0.000 description 4
- 150000003512 tertiary amines Chemical class 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 3
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 3
- VNWOJVJCRAHBJJ-UHFFFAOYSA-N 2-pentylcyclopentan-1-one Chemical compound CCCCCC1CCCC1=O VNWOJVJCRAHBJJ-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 239000005062 Polybutadiene Substances 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 3
- 239000001110 calcium chloride Substances 0.000 description 3
- 229910001628 calcium chloride Inorganic materials 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 150000001993 dienes Chemical class 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000005227 gel permeation chromatography Methods 0.000 description 3
- 150000002460 imidazoles Chemical class 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 238000010030 laminating Methods 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910000000 metal hydroxide Inorganic materials 0.000 description 3
- 150000004692 metal hydroxides Chemical class 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 229920002857 polybutadiene Polymers 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 150000003141 primary amines Chemical class 0.000 description 3
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 3
- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- MSFGZHUJTJBYFA-UHFFFAOYSA-M sodium dichloroisocyanurate Chemical compound [Na+].ClN1C(=O)[N-]C(=O)N(Cl)C1=O MSFGZHUJTJBYFA-UHFFFAOYSA-M 0.000 description 3
- 230000001629 suppression Effects 0.000 description 3
- 230000004580 weight loss Effects 0.000 description 3
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 description 2
- ZGEGCLOFRBLKSE-UHFFFAOYSA-N 1-Heptene Chemical compound CCCCCC=C ZGEGCLOFRBLKSE-UHFFFAOYSA-N 0.000 description 2
- IANQTJSKSUMEQM-UHFFFAOYSA-N 1-benzofuran Chemical compound C1=CC=C2OC=CC2=C1 IANQTJSKSUMEQM-UHFFFAOYSA-N 0.000 description 2
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 description 2
- KWKAKUADMBZCLK-UHFFFAOYSA-N 1-octene Chemical compound CCCCCCC=C KWKAKUADMBZCLK-UHFFFAOYSA-N 0.000 description 2
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 description 2
- YBYIRNPNPLQARY-UHFFFAOYSA-N 1H-indene Chemical compound C1=CC=C2CC=CC2=C1 YBYIRNPNPLQARY-UHFFFAOYSA-N 0.000 description 2
- WZYHGSHVTXRAFY-UHFFFAOYSA-N 2,2-dimethylimidazole Chemical compound CC1(C)N=CC=N1 WZYHGSHVTXRAFY-UHFFFAOYSA-N 0.000 description 2
- GQHTUMJGOHRCHB-UHFFFAOYSA-N 2,3,4,6,7,8,9,10-octahydropyrimido[1,2-a]azepine Chemical compound C1CCCCN2CCCN=C21 GQHTUMJGOHRCHB-UHFFFAOYSA-N 0.000 description 2
- SDJHPPZKZZWAKF-UHFFFAOYSA-N 2,3-dimethylbuta-1,3-diene Chemical compound CC(=C)C(C)=C SDJHPPZKZZWAKF-UHFFFAOYSA-N 0.000 description 2
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 description 2
- UHKPXKGJFOKCGG-UHFFFAOYSA-N 2-methylprop-1-ene;styrene Chemical compound CC(C)=C.C=CC1=CC=CC=C1.C=CC1=CC=CC=C1 UHKPXKGJFOKCGG-UHFFFAOYSA-N 0.000 description 2
- XMTQQYYKAHVGBJ-UHFFFAOYSA-N 3-(3,4-DICHLOROPHENYL)-1,1-DIMETHYLUREA Chemical compound CN(C)C(=O)NC1=CC=C(Cl)C(Cl)=C1 XMTQQYYKAHVGBJ-UHFFFAOYSA-N 0.000 description 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 244000260524 Chrysanthemum balsamita Species 0.000 description 2
- 235000005633 Chrysanthemum balsamita Nutrition 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 229920002367 Polyisobutene Polymers 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- 229920000180 alkyd Polymers 0.000 description 2
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 229920006026 co-polymeric resin Polymers 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000000113 differential scanning calorimetry Methods 0.000 description 2
- ZZTCPWRAHWXWCH-UHFFFAOYSA-N diphenylmethanediamine Chemical compound C=1C=CC=CC=1C(N)(N)C1=CC=CC=C1 ZZTCPWRAHWXWCH-UHFFFAOYSA-N 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000009545 invasion Effects 0.000 description 2
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 229940018564 m-phenylenediamine Drugs 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 150000005673 monoalkenes Chemical class 0.000 description 2
- 229920003986 novolac Polymers 0.000 description 2
- UTOPWMOLSKOLTQ-UHFFFAOYSA-N octacosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCC(O)=O UTOPWMOLSKOLTQ-UHFFFAOYSA-N 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 2
- 150000003003 phosphines Chemical class 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 239000010734 process oil Substances 0.000 description 2
- 238000007348 radical reaction Methods 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 150000003335 secondary amines Chemical class 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229920002050 silicone resin Polymers 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- 239000002562 thickening agent Substances 0.000 description 2
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 2
- 239000001993 wax Substances 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- LTQBNYCMVZQRSD-UHFFFAOYSA-N (4-ethenylphenyl)-trimethoxysilane Chemical compound CO[Si](OC)(OC)C1=CC=C(C=C)C=C1 LTQBNYCMVZQRSD-UHFFFAOYSA-N 0.000 description 1
- AILUJKZWHGGGRF-UHFFFAOYSA-M (4-methylphenyl)-triphenylphosphanium;thiocyanate Chemical compound [S-]C#N.C1=CC(C)=CC=C1[P+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 AILUJKZWHGGGRF-UHFFFAOYSA-M 0.000 description 1
- RUEBPOOTFCZRBC-UHFFFAOYSA-N (5-methyl-2-phenyl-1h-imidazol-4-yl)methanol Chemical compound OCC1=C(C)NC(C=2C=CC=CC=2)=N1 RUEBPOOTFCZRBC-UHFFFAOYSA-N 0.000 description 1
- PMJHHCWVYXUKFD-SNAWJCMRSA-N (E)-1,3-pentadiene Chemical compound C\C=C\C=C PMJHHCWVYXUKFD-SNAWJCMRSA-N 0.000 description 1
- GIWQSPITLQVMSG-UHFFFAOYSA-N 1,2-dimethylimidazole Chemical compound CC1=NC=CN1C GIWQSPITLQVMSG-UHFFFAOYSA-N 0.000 description 1
- FBHPRUXJQNWTEW-UHFFFAOYSA-N 1-benzyl-2-methylimidazole Chemical compound CC1=NC=CN1CC1=CC=CC=C1 FBHPRUXJQNWTEW-UHFFFAOYSA-N 0.000 description 1
- XZKLXPPYISZJCV-UHFFFAOYSA-N 1-benzyl-2-phenylimidazole Chemical compound C1=CN=C(C=2C=CC=CC=2)N1CC1=CC=CC=C1 XZKLXPPYISZJCV-UHFFFAOYSA-N 0.000 description 1
- OQJQPIWVCBJVAZ-UHFFFAOYSA-N 1-methyl-2-phenylimidazole Chemical compound CN1C=CN=C1C1=CC=CC=C1 OQJQPIWVCBJVAZ-UHFFFAOYSA-N 0.000 description 1
- SEULWJSKCVACTH-UHFFFAOYSA-N 1-phenylimidazole Chemical compound C1=NC=CN1C1=CC=CC=C1 SEULWJSKCVACTH-UHFFFAOYSA-N 0.000 description 1
- VHJRQDUWYYJDBE-UHFFFAOYSA-N 11-trimethoxysilylundecane-1-thiol Chemical compound CO[Si](OC)(OC)CCCCCCCCCCCS VHJRQDUWYYJDBE-UHFFFAOYSA-N 0.000 description 1
- 238000005160 1H NMR spectroscopy Methods 0.000 description 1
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 1
- PISLZQACAJMAIO-UHFFFAOYSA-N 2,4-diethyl-6-methylbenzene-1,3-diamine Chemical compound CCC1=CC(C)=C(N)C(CC)=C1N PISLZQACAJMAIO-UHFFFAOYSA-N 0.000 description 1
- STMDPCBYJCIZOD-UHFFFAOYSA-N 2-(2,4-dinitroanilino)-4-methylpentanoic acid Chemical compound CC(C)CC(C(O)=O)NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O STMDPCBYJCIZOD-UHFFFAOYSA-N 0.000 description 1
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 description 1
- FPZWZCWUIYYYBU-UHFFFAOYSA-N 2-(2-ethoxyethoxy)ethyl acetate Chemical compound CCOCCOCCOC(C)=O FPZWZCWUIYYYBU-UHFFFAOYSA-N 0.000 description 1
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- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- 229940014800 succinic anhydride Drugs 0.000 description 1
- TXDNPSYEJHXKMK-UHFFFAOYSA-N sulfanylsilane Chemical compound S[SiH3] TXDNPSYEJHXKMK-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- DDFYFBUWEBINLX-UHFFFAOYSA-M tetramethylammonium bromide Chemical compound [Br-].C[N+](C)(C)C DDFYFBUWEBINLX-UHFFFAOYSA-M 0.000 description 1
- GHPYAGKTTCKKDF-UHFFFAOYSA-M tetraphenylphosphanium;thiocyanate Chemical compound [S-]C#N.C1=CC=CC=C1[P+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 GHPYAGKTTCKKDF-UHFFFAOYSA-M 0.000 description 1
- AYEKOFBPNLCAJY-UHFFFAOYSA-O thiamine pyrophosphate Chemical compound CC1=C(CCOP(O)(=O)OP(O)(O)=O)SC=[N+]1CC1=CN=C(C)N=C1N AYEKOFBPNLCAJY-UHFFFAOYSA-O 0.000 description 1
- 150000003557 thiazoles Chemical class 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000000411 transmission spectrum Methods 0.000 description 1
- 150000003918 triazines Chemical class 0.000 description 1
- FBBATURSCRIBHN-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyldisulfanyl)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCSSCCC[Si](OCC)(OCC)OCC FBBATURSCRIBHN-UHFFFAOYSA-N 0.000 description 1
- VTHOKNTVYKTUPI-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyltetrasulfanyl)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCSSSSCCC[Si](OCC)(OCC)OCC VTHOKNTVYKTUPI-UHFFFAOYSA-N 0.000 description 1
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 description 1
- NMEPHPOFYLLFTK-UHFFFAOYSA-N trimethoxy(octyl)silane Chemical compound CCCCCCCC[Si](OC)(OC)OC NMEPHPOFYLLFTK-UHFFFAOYSA-N 0.000 description 1
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- QLAGHGSFXJZWKY-UHFFFAOYSA-N triphenylborane;triphenylphosphane Chemical compound C1=CC=CC=C1B(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 QLAGHGSFXJZWKY-UHFFFAOYSA-N 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 229940099259 vaseline Drugs 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
- H01L23/293—Organic, e.g. plastic
- H01L23/295—Organic, e.g. plastic containing a filler
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/31—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the arrangement or shape
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
- H01L31/042—PV modules or arrays of single PV cells
- H01L31/048—Encapsulation of modules
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
- H01L31/042—PV modules or arrays of single PV cells
- H01L31/048—Encapsulation of modules
- H01L31/0481—Encapsulation of modules characterised by the composition of the encapsulation material
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/02—Details
- H05B33/04—Sealing arrangements, e.g. against humidity
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/204—Applications use in electrical or conductive gadgets use in solar cells
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/844—Encapsulations
Abstract
The present invention provides a resin composition and a resin sheet using the same, wherein the resin composition comprises a polyolefin resin and a semi-calcined hydrotalcite, the content of the semi-calcined hydrotalcite exceeds 45 mass% relative to 100 mass% of a nonvolatile component of the resin composition, and the water content is 2500ppm or less based on the mass of the whole resin composition.
Description
Technical Field
The present invention relates to a resin composition useful for sealing electronic devices and a resin sheet using the same.
Background
In order to protect electronic devices such as organic EL (Electroluminescence) devices and solar cells from moisture, sealing of the electronic devices is performed using the resin composition.
As a resin composition suitable for sealing an electronic device, a composition containing a hygroscopic filler in a resin composition is known. For example, patent document 1 discloses a sealing resin composition containing a hygroscopic metal hydroxide, and a sealing sheet comprising a support and a resin composition layer formed of the sealing resin composition.
Documents of the prior art
Patent document
Patent document 1: international publication No. 2017/057708.
Disclosure of Invention
Technical problem to be solved by the invention
In the field of electronic devices, there is a continuous demand for improvement in sealing performance (specifically, performance of suppressing deterioration of a portion to be sealed) of a resin composition used for sealing an electronic device. The resin composition comprising the polyolefin-based resin and the semi-calcined hydrotalcite is excellent in moisture permeation resistance and transparency, and can be used for sealing electronic devices. However, the following problems have been found: if the content of the semi-calcined hydrotalcite in the resin composition is increased in order to improve moisture permeation resistance, deterioration of the site to be sealed with time increases despite the increase in the content of the semi-calcined hydrotalcite as a hygroscopic filler, and there is a limit to improvement of sealing performance. The present invention has been made in view of such circumstances, and an object thereof is to provide a resin composition having excellent sealing performance and a resin sheet using the same.
Technical scheme for solving technical problem
As a result of earnest studies, the present inventors have found that the moisture trapped in the semi-calcined hydrotalcite reaches the site to be sealed with the passage of time, and causes the deterioration thereof, and if the content of the semi-calcined hydrotalcite is increased, the deterioration becomes remarkable. Further, it has been found that, in order to improve sealing performance, the moisture permeability resistance is improved by increasing the content of the semi-calcined hydrotalcite, and the sealing performance (moisture permeability resistance and suppression of deterioration of a sealing target portion due to internal moisture) can be improved by decreasing the amount of internal moisture in the resin composition introduced by the semi-calcined hydrotalcite.
The present invention based on the above findings is as follows;
[1] a resin composition comprising a polyolefin-based resin and a semi-calcined hydrotalcite, wherein the semi-calcined hydrotalcite is contained in an amount of more than 45% by mass based on 100% by mass of nonvolatile components of the resin composition and has a water content of 2500ppm or less based on the mass of the entire resin composition;
[2] the resin composition according to the above [1], wherein the water content is 2000ppm or less on a mass basis with respect to the entire resin composition;
[3] the resin composition according to [1] or [2], wherein the content of the semi-calcined hydrotalcite is more than 45% by mass and 80% by mass or less with respect to 100% by mass of nonvolatile components of the resin composition;
[4] the resin composition according to any one of the above [1] to [3], wherein the resin composition is used for sealing an electronic device;
[5] the resin composition according to the above [4], wherein the electronic device is an organic EL device or a solar cell;
[6] a resin sheet comprising a support and a layer of the resin composition according to any one of the above [1] to [3] provided on the support;
[7] the resin sheet according to the above [6], wherein the resin sheet is used for sealing an electronic device;
[8] the resin sheet according to the above [7], wherein the electronic device is an organic EL device or a solar cell.
ADVANTAGEOUS EFFECTS OF INVENTION
According to the present invention, a resin composition excellent in sealing performance of an electronic device and a resin sheet using the same can be obtained.
Detailed Description
The present invention will be described below in order. The examples and preferred embodiments described below can be combined with each other as long as they are not contradictory to each other.
< resin composition >
The resin composition of the present invention comprises a polyolefin-based resin and a semi-calcined hydrotalcite. The sealing layer formed of the resin composition containing the semi-calcined hydrotalcite absorbs moisture in the outside air, and therefore can suppress deterioration of the electronic device due to moisture entering from the outside air.
However, in the sealing layer formed of the resin composition containing the semi-calcined hydrotalcite, moisture (which may be interlayer water of the semi-calcined hydrotalcite and moisture adhering to the surface of the semi-calcined hydrotalcite) trapped by the semi-calcined hydrotalcite is taken into the sealing layer, and this moisture reaches the electronic device with the passage of time, which is a factor causing deterioration of the electronic device.
Therefore, it is found that it is difficult to improve the sealing performance of the resin composition by simply increasing the amount of the semi-calcined hydrotalcite used. Further, the present inventors have studied and found that the above-mentioned problems cannot be solved even when the semi-calcined hydrotalcite is incorporated into a resin composition by drying it in advance. The reason for this is presumed to be that the semi-calcined hydrotalcite, even after drying, immediately captures moisture in the air and returns to its original state. Therefore, it is necessary to dry the resin composition containing the semi-calcined hydrotalcite so that the moisture contained in the resin composition is reduced to a certain value or less.
Even when the amount of the semi-calcined hydrotalcite to be used is increased in order to improve moisture permeability resistance, the water content of the resin composition containing the semi-calcined hydrotalcite is sufficiently reduced, whereby deterioration of electronic devices due to moisture in the resin composition introduced by the semi-calcined hydrotalcite is sufficiently suppressed, and a resin composition having excellent sealing performance can be provided. One of the features of the present invention based on this finding is that the water content of the resin composition is 2500ppm or less based on the mass of the entire resin composition (the entire resin composition including volatile components and nonvolatile components). The lower the water content is, the better the water content is (preferably 0ppm), the more preferably 2000ppm or less, the more preferably 1500ppm or less, the further preferably 1000ppm or less, and particularly preferably 800ppm or less. The water content can be measured as described in the following examples.
The water content of 2500ppm or less can be achieved by appropriately setting the drying conditions of the resin composition. For example, when the varnish of the resin composition is applied to the support and heated to form the resin composition layer, the resin composition layer is formed by setting the heating temperature (i.e., the heating temperature of the coating film formed by the varnish application) at which the resin composition layer is formed to 70 to 150 ℃ and the heating time to 10 minutes to 2 hours, and then the formed resin composition layer is additionally dried at the drying temperature (heating temperature) of 100 to 180 ℃ and the drying time to 10 minutes to 7 weeks, whereby the water content of the resin composition layer can be made 2500ppm or less.
When the heating temperature for forming the resin composition layer and additional drying thereafter is low, it may take a long time to make the water content of the resin composition to 2500ppm or less, or it may be difficult to make the water content of the resin composition to 2500ppm or less. Therefore, the heating temperature for forming the resin composition layer and the subsequent additional drying is preferably a high temperature to some extent. However, if the heating temperature is set too high in the formation of the resin composition layer, there is a possibility that air bubbles may enter the resin composition layer. Therefore, it is preferable that the formation temperature of the resin composition layer is set relatively low, and the temperature for additional drying of the subsequent resin composition layer is set higher than the formation temperature of the resin composition layer.
< polyolefin-based resin >
The polyolefin-based resin that can be used in the present invention is not particularly limited as long as it has a skeleton derived from an olefin. For example, as the polyolefin resin described in patent document 1, known resins can be cited. The olefin is preferably a monoolefin having 1 olefinic carbon-carbon double bond and/or a diolefin having 2 olefinic carbon-carbon double bonds. Preferred examples of the monoolefin include α -olefins such as ethylene, propylene, 1-butene, isobutylene, 1-pentene, 1-hexene, 1-heptene and 1-octene; preferable examples of the diene include 1, 3-butadiene, isoprene, 1, 3-pentadiene, and 2, 3-dimethylbutadiene. The polyolefin-based resin may have 1 or 2 or more olefin-derived skeletons. The polyolefin-based resin may be used in only 1 kind, or 2 or more kinds may be used in combination.
The polyolefin-based resin may be a homopolymer, or a copolymer such as a random copolymer or a block copolymer. Examples of the copolymer include a copolymer of 2 or more kinds of olefins and a copolymer of an olefin and a monomer other than olefins such as a non-conjugated diene and styrene. Examples of preferable copolymers include ethylene-nonconjugated diene copolymers, ethylene-propylene-nonconjugated diene copolymers, ethylene-butene copolymers, propylene-butene-nonconjugated diene copolymers, styrene-isobutylene-styrene copolymers, and the like.
Examples of the polyolefin resin include an isobutylene-modified resin described in international publication No. 2011/62167 and a styrene-isobutylene-modified resin described in international publication No. 2013/108731.
The polyolefin-based resin is preferably a polybutene-based resin or a polypropylene-based resin. Here, the "polybutene-based resin" refers to a resin in which the main unit (the largest content unit) of all the olefin monomer units constituting the polymer is derived from butene, and the "polypropylene-based resin" refers to a resin in which the main unit (the largest content unit) of all the olefin monomer units constituting the polymer is derived from propylene.
When the polybutene-based resin is a copolymer, examples of the monomer other than butene include styrene, ethylene, propylene, and isoprene. When the polypropylene-based resin is a copolymer, examples of the monomer other than propylene include ethylene, butene, and isoprene.
From the viewpoint of imparting excellent physical properties such as adhesiveness and adhesive moisture and heat resistance, the polyolefin-based resin preferably contains: a polyolefin-based resin having an acid anhydride group (i.e., carbonyloxycarbonyl group (-CO-O-CO-)) and/or a polyolefin-based resin having an epoxy group. Examples of the acid anhydride group include a group derived from succinic anhydride, a group derived from maleic anhydride, and a group derived from glutaric anhydride. The polyolefin-based resin may have 1 or 2 or more kinds of acid anhydride groups. The polyolefin-based resin having an acid anhydride group can be obtained, for example, by graft-modifying a polyolefin-based resin with an unsaturated compound having an acid anhydride group under radical reaction conditions. Further, the unsaturated compound having an acid anhydride group may be subjected to radical copolymerization together with an olefin or the like. Similarly, the polyolefin-based resin having an epoxy group can be obtained by graft-modifying an unsaturated compound having an epoxy group such as glycidyl (meth) acrylate, 4-hydroxybutyl acrylate glycidyl ether, allyl glycidyl ether or the like under a radical reaction condition. In addition, an unsaturated compound having an epoxy group may be subjected to radical copolymerization together with an olefin or the like. The polyolefin-based resin may be used in 1 kind or 2 or more kinds, and the polyolefin-based resin having an acid anhydride group and the polyolefin-based resin having an epoxy group may be used in combination.
As the polyolefin-based resin having an acid anhydride group, a polybutene-based resin having an acid anhydride group and a polypropylene-based resin having an acid anhydride group are preferred. Further, as the polyolefin resin having an epoxy group, a polybutene resin having an epoxy group and a polypropylene resin having an epoxy group are preferable.
The concentration of the acid anhydride group in the polyolefin-based resin having an acid anhydride group is preferably 0.05 to 10mmol/g, more preferably 0.1 to 5 mmol/g. The concentration of the acid anhydride group is obtained from the value defined as the acid value of mg of potassium hydroxide required for neutralizing the acid present in 1g of the resin in accordance with JIS K2501. The amount of the polyolefin-based resin having an acid anhydride group in the polyolefin-based resin is preferably 0 to 70% by mass, more preferably 10 to 50% by mass.
In addition, the concentration of the epoxy group in the polyolefin-based resin having an epoxy group is preferably 0.05 to 10mmol/g, more preferably 0.1 to 5 mmol/g. The epoxy group concentration was determined from the epoxy equivalent obtained in accordance with JIS K7236-1995. In addition, the amount of the polyolefin-based resin having an epoxy group in the polyolefin-based resin is preferably 0 to 70% by mass, more preferably 10 to 50% by mass.
The polyolefin-based resin is particularly preferably a polyolefin-based resin containing both an acid anhydride group-containing polyolefin-based resin and an epoxy group-containing polyolefin-based resin from the viewpoint of imparting excellent physical properties such as sealing performance. Such polyolefin-based resin can form a sealing layer having excellent sealing performance and the like by forming a crosslinked structure by reacting an acid anhydride group and an epoxy group by heating. The formation of the crosslinked structure may be performed after the sealing, but in the case where the resistance to heat of the object to be sealed such as an electronic device is weak, for example, it is desirable to seal with a sealing film and to form the crosslinked structure in advance at the time of manufacturing the sealing film.
The ratio of the polyolefin-based resin having an acid anhydride group to the polyolefin-based resin having an epoxy group is not particularly limited as long as an appropriate crosslinked structure can be formed, and the molar ratio of the epoxy group to the acid anhydride group (epoxy group: acid anhydride group) is preferably 100:10 to 100:400, more preferably 100:25 to 100:350, particularly preferably 100:40 to 100: 300.
In the resin composition of the present invention, in the case of using a polyolefin-based resin having an epoxy group, a polyolefin-based resin having a functional group reactive with the epoxy group (except for an acid anhydride group) can be used. Examples of the functional group include a hydroxyl group, a phenolic hydroxyl group, an amino group, and a carboxyl group.
In the case of using a polyolefin-based resin having an acid anhydride group in the resin composition of the present invention, a polyolefin-based resin having a functional group reactive with an acid anhydride group (excluding an epoxy group) can be used. Examples of the functional group include a hydroxyl group, a primary or secondary amino group, a mercapto group, and an oxetanyl group.
The number average molecular weight of the polyolefin-based resin is not particularly limited, but is preferably 1000000 or less, more preferably 750000 or less, further preferably 500000 or less, further preferably 400000 or less, further more preferably 300000 or less, particularly preferably 200000 or less, and most preferably 150000 or less, from the viewpoint of providing a varnish of the resin composition with good coatability and good compatibility with other components in the resin composition. On the other hand, the number average molecular weight is preferably 1000 or more, more preferably 2000 or more, from the viewpoint of preventing sagging at the time of coating the varnish of the resin composition, exerting the sealing performance of the formed resin composition layer, and improving the mechanical strength. The number average molecular weight in the present invention is measured by a Gel Permeation Chromatography (GPC) method (polystyrene conversion). Specifically, the number average molecular weight measured by GPC was measured at a column temperature of 40 ℃ using LC-9A/RID-6A manufactured by Shimadzu corporation as a measuring apparatus, Shodex K-800P/K-804L/K-804L manufactured by Showa Denko K.K., toluene or the like as a mobile phase, and a calibration curve of standard polystyrene was calculated.
The polyolefin-based resin in the present invention is preferably amorphous from the viewpoint of suppressing the decrease in fluidity due to thickening of the varnish. Herein, non-crystalline means that the polyolefin-based resin does not have a clear melting point, and for example, a resin in which a clear peak is not observed when the melting point of the polyolefin-based resin is measured by DSC (differential scanning calorimetry) can be used.
Next, specific examples of the polyolefin-based resin will be described. Specific examples of the polypropylene-based resin include: "T-YP 341" (glycidyl methacrylate-modified propylene-butene random copolymer, available from Shikuwa PMC Co., Ltd., the amount of butene units based on 100 mass% of the total of propylene units and butene units: 29 mass%, epoxy group concentration: 0.638mmol/g, number average molecular weight: 155000), "T-YP 279" (maleic anhydride-modified propylene-butene random copolymer, available from Shikuwa PMC Co., Ltd., the amount of butene units based on 100 mass% of the total of propylene units and butene units: 36 mass%, acid anhydride group concentration: 0.464mmol/g, number average molecular weight: 35000), and "T-YP 276" (glycidyl methacrylate-modified propylene-butene random copolymer, the amount of butene units based on 100 mass% of the total of propylene units and butene units: 36 mass%, epoxy group concentration: 0.638mmol/g, number average molecular weight: 57000) "T-YP 312" (maleic anhydride-modified propylene-butene random copolymer, amount of butene units based on 100 mass% of the total of propylene units and butene units: 29 mass%, acid anhydride group concentration: 0.464mmol/g, number average molecular weight: 60900) "T-YP 313" manufactured by seiko PMC corporation (glycidyl methacrylate-modified propylene-butene random copolymer, amount of butene unit based on 100 mass% of the total of propylene unit and butene unit: 29 mass%, epoxy group concentration: 0.638mmol/g, number average molecular weight: 155000), etc.
Specific examples of the polybutene-based resin include: "HV-1900" (polybutene, number average molecular weight: 2900) manufactured by ENEOS corporation (old name "JXTG energy Co., Ltd."), "HV-300M" (modified product of maleic anhydride-modified liquid polybutene ("HV-300" (number average molecular weight: 1400)) manufactured by Toho chemical industries, number average molecular weight: 2100, number of carboxyl groups constituting an acid anhydride group: 3.2/1 molecule, acid value: 43.4mgKOH/g, acid anhydride group concentration: 0.77mmol/g), "OPPANOL B100" (polyisobutylene, viscosity average molecular weight: 1110000) manufactured by Basff corporation, and "N50 SF" (polyisobutylene, viscosity average molecular weight: 400000) manufactured by Basff corporation.
Specific examples of the styrene-isobutylene copolymer include: "SIBSTAR T102" (styrene-isobutylene-styrene block copolymer, number average molecular weight: 100000, styrene content: 30 mass%) manufactured by Kaneka corporation, and "T-YP 757B" (maleic anhydride-modified styrene-isobutylene-styrene block copolymer, acid anhydride group concentration: 0.464mmol/g, number average molecular weight: 100000) manufactured by Astroluminescent PMC corporation, "T-YP 766" (glycidyl methacrylate-modified styrene-isobutylene-styrene block copolymer, epoxy group concentration: 0.638mmol/g, number average molecular weight: 100000) manufactured by Astroluminescent PMC corporation, and "T-YP 8920" (maleic anhydride-modified styrene-isobutylene-styrene copolymer, acid anhydride group concentration: 0.464mmol/g, number average molecular weight: 35800) manufactured by Astroluminescent PMC corporation, and "T-YP 8930" (glycidyl methacrylate-modified styrene-isobutylene-styrene block copolymer, number average molecular weight: 35800) manufactured by Astroluminescent PMC corporation Styrene copolymer, epoxy group concentration: 0.638mmol/g, number average molecular weight: 48700).
The content of the polyolefin-based resin in the resin composition of the present invention is not particularly limited. However, from the viewpoint of sealing performance and handling properties of the resin composition, the content is preferably 5% by mass or more, more preferably 10% by mass or more, further preferably 15% by mass or more, preferably 50% by mass or less, further preferably 40% by mass or less, further preferably 35% by mass or less, relative to 100% by mass of the nonvolatile component of the resin composition.
< semi-calcined hydrotalcite >
Hydrotalcites can be classified into uncalcined hydrotalcites, semi-calcined hydrotalcites and calcined hydrotalcites. The semi-calcined hydrotalcite is used in the present invention from the viewpoint of transparency and moisture permeation resistance of the resin composition.
The uncalcined hydrotalcite may be, for example, a natural hydrotalcite (Mg)6Al2(OH)16CO3·4H2O) a metal hydroxide having a layered crystal structure, represented by, for example, a layer [ Mg ] as a basic skeleton1-XAlX(OH)2]X+And an intermediate layer [ (CO)3)X/2·mH2O]X-And (4) forming. The uncalcined hydrotalcite in the present invention is a concept of hydrotalcite-like compound including synthetic hydrotalcite and the like. Examples of the hydrotalcite-like compound include compounds represented by the following formula (I) and the following formula (II).
[M2+ 1-xM3+ x(OH)2]x+·[(An-)x/n·mH2O]x- (I)
(in the formula, M2+Represents Mg2+、Zn2+Isovalent 2 metal ion, M3+Represents Al3+、Fe3+Isovalent 3 metal ion, An-Represents CO3 2-、Cl-、NO3 -Equal n-valent anions, x is more than 0 and less than 1, m is more than or equal to 0 and less than 1, and n is a positive number. )
In the formula (I), M2+Preferably Mg2+,M3+Preferably Al3+,An-Preferably CO3 2-。
M2+ xAl2(OH)2x+6-nz(An-)z·mH2O (II)
(in the formula, M2+Represents Mg2+、Zn2+Isovalent 2 metal ion, An-Represents CO3 2-、Cl-、NO3 -An n-valent anion, x is a positive number of 2 or more, z is a positive number of 2 or less, m is a positive number, and n is a positive number. )
In the formula (II), M2+Preferably Mg2+,An-Preferably CO3 2-。
Semi-calcinationHydrotalcite refers to a metal hydroxide having a layered crystal structure in which the amount of interlayer water is reduced or eliminated, which is obtained by calcining uncalcined hydrotalcite. The term "interlayer water" as used herein means "H" described in the above-mentioned compositional formula of the uncalcined natural hydrotalcite and hydrotalcite-like compound2O”。
On the other hand, calcined hydrotalcite is a metal oxide having an amorphous structure, which is obtained by calcining uncalcined hydrotalcite or semi-calcined hydrotalcite and in which not only interlayer water but also hydroxyl groups disappear by condensation dehydration.
The uncalcined hydrotalcite, semi-calcined hydrotalcite and calcined hydrotalcite may be distinguished by saturated water absorption. The saturated water absorption of the semi-calcined hydrotalcite is 1 mass% or more and less than 20 mass%. On the other hand, the non-calcined hydrotalcite has a saturated water absorption of less than 1 mass%, and the calcined hydrotalcite has a saturated water absorption of 20 mass% or more.
The "saturated water absorption" in the present invention means: a measurement sample (for example, half-calcined hydrotalcite) 1.5g was weighed out using a balance, and after measuring the initial mass, the sample was allowed to stand for 200 hours under atmospheric pressure in a small environmental tester (SH-222 manufactured by ESPEC) set at 60 ℃ and 90% RH (relative humidity), and the rate of increase in mass of the sample after standing for 200 hours from the initial mass was determined by the following formula (i):
saturated water absorption (mass%) is 100 × (mass after moisture absorption-initial mass)/initial mass (i).
The saturated water absorption of the semi-calcined hydrotalcite is preferably 3 mass% or more and less than 20 mass%, more preferably 5 mass% or more and less than 20 mass%.
Furthermore, the uncalcined hydrotalcite, the semi-calcined hydrotalcite and the calcined hydrotalcite can be distinguished by the thermogravimetric reduction rate measured by thermogravimetric analysis. The rate of decrease in thermogravimetric quantity at 280 ℃ of the semi-calcined hydrotalcite is less than 15 mass%, and the rate of decrease in thermogravimetric quantity at 380 ℃ is 12 mass% or more. On the other hand, the weight loss rate at 280 ℃ of the uncalcined hydrotalcite was 15% by mass or more, and the weight loss rate at 380 ℃ of the calcined hydrotalcite was less than 12% by mass.
For thermogravimetric analysis, 5mg of hydrotalcite was weighed into an aluminum sample tray using TG/DTAEXSTAR6300 manufactured by Hitach High-Tech Science, and the weighing was carried out under conditions of a temperature rise rate of 10 ℃/min from 30 ℃ to 550 ℃ in an open state without a lid under a nitrogen flow rate of 200 mL/min. The thermogravimetric reduction rate can be obtained by the following formula (ii):
the weight loss rate (mass%) of heat was 100 × (mass before heating-mass at a predetermined temperature)/mass before heating (ii).
Furthermore, the uncalcined hydrotalcite, the semi-calcined hydrotalcite and the calcined hydrotalcite may be distinguished by the peak and relative intensity ratio as measured by powder X-ray diffraction. The semi-calcined hydrotalcite exhibits a peak split into two peaks by powder X-ray diffraction at around 8-18 DEG 2 [ theta ], or exhibits a peak having a shoulder peak by synthesis of two peaks, and the relative intensity ratio (low-angle side diffraction intensity/high-angle side diffraction intensity) between the diffraction intensity of a peak or shoulder peak appearing on the low-angle side (low-angle side diffraction intensity) and the diffraction intensity of a peak or shoulder peak appearing on the high-angle side (high-angle side diffraction intensity) is 0.001-1,000. On the other hand, the uncalcined hydrotalcite has only one peak in the vicinity of 8 to 18 °, or the relative intensity ratio of the diffraction intensity of the peak or shoulder appearing on the low angle side to the peak or shoulder appearing on the high angle side falls outside the aforementioned range. The calcined hydrotalcite has no characteristic peak in the region of 8 ° to 18 ° and has a characteristic peak at 43 °. For the powder X-ray diffraction measurement, CuK alpha was measured at the counter cathode using a powder X-ray diffraction apparatus (Empyrean, manufactured by PANALYtic Co., Ltd.)Under the conditions that the voltage is 45V, the current is 40mA, the sampling width is 0.0260 degree, the scanning speed is 0.0657 degrees/s, and the diffraction angle range (2 theta) is 5.0131-79.9711 degrees. The Peak search (Peak search) can be performed under the conditions of "the minimum degree of significance is 0.50, the minimum Peak Tip (Peak Tip) is 0.01 °, the maximum Peak Tip is 1.00 °, the Peak base width is 2.00 °, and the method is the minimum value of the second order differential" by using the Peak search function of software attached to the diffraction device.
The BET specific surface area of the semi-calcined hydrotalcite and the calcined hydrotalcite is preferably 1-250 m2A specific ratio of the total amount of the compound to the total amount of the compound is 5 to 200m2(iv) g. The BET specific surface areas of these compounds can be calculated by the BET multipoint method by adsorbing nitrogen gas onto the surface of a sample using a specific surface area measuring apparatus (Macsorb HM 1210, manufactured by MOUNTECH Co., Ltd.).
The particle size of the semi-calcined hydrotalcite is preferably 1 to 1000nm, more preferably 10 to 800 nm. The particle diameter is a median diameter of a particle size distribution obtained by preparing a particle size distribution on a volume basis by laser diffraction scattering particle size distribution measurement (JIS Z8825).
The semi-calcined hydrotalcite may be a material surface-treated with a surface treatment agent. As the surface treatment agent used for the surface treatment, for example, higher fatty acids, alkylsilanes, silane coupling agents, and the like can be used, and among them, higher fatty acids and alkylsilanes are preferable. The surface treatment agent may be used in 1 kind or 2 kinds or more.
Examples of the higher fatty acid include higher fatty acids having 18 or more carbon atoms such as stearic acid, montanic acid, myristic acid, palmitic acid, etc., and stearic acid is particularly preferable. These may be used in 1 or 2 or more.
Examples of the alkylsilanes include: methyltrimethoxysilane, ethyltrimethoxysilane, hexyltrimethoxysilane, octyltrimethoxysilane, decyltrimethoxysilane, octadecyltrimethoxysilane, dimethyldimethoxysilane, octyltriethoxysilane, n-octadecyl dimethyl (3- (trimethoxysilyl) propyl) ammonium chloride, etc. These may be used in 1 or 2 or more.
Examples of the silane coupling agent include: epoxy silane coupling agents such as 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropyltriethoxysilane, 3-glycidoxypropyl (dimethoxy) methylsilane and 2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane; mercapto silane coupling agents such as 3-mercaptopropyltrimethoxysilane, 3-mercaptopropyltriethoxysilane, 3-mercaptopropylmethyldimethoxysilane and 11-mercaptoundecyltrimethoxysilane; amino silane coupling agents such as 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, 3-aminopropyldimethoxymethylsilane, N-phenyl-3-aminopropyltrimethoxysilane, N-methylaminopropyltrimethoxysilane, N- (2-aminoethyl) -3-aminopropyltrimethoxysilane and N- (2-aminoethyl) -3-aminopropyldimethoxymethylsilane; ureido-based silane coupling agents such as 3-ureidopropyltriethoxysilane; vinyl silane coupling agents such as vinyltrimethoxysilane, vinyltriethoxysilane and vinylmethyldiethoxysilane; styrene-based silane coupling agents such as p-styryltrimethoxysilane; acrylate-based silane coupling agents such as 3-acryloxypropyltrimethoxysilane and 3-methacryloxypropyltrimethoxysilane; isocyanate-based silane coupling agents such as 3-isocyanatopropyltrimethoxysilane; sulfide-based silane coupling agents such as bis (triethoxysilylpropyl) disulfide and bis (triethoxysilylpropyl) tetrasulfide; phenyltrimethoxysilane, methacryloxypropyltrimethoxysilane, imidazolesilane, triazinesilane and the like. These may be used in 1 or 2 or more.
The surface treatment of the semi-calcined hydrotalcite or the like can be carried out, for example, by: while stirring and dispersing untreated semi-calcined hydrotalcite or the like at normal temperature using a mixer, the surface treatment agent is added by spraying and stirred for 5 to 60 minutes. As the mixer, a known mixer can be used, and examples thereof include a mixer such as a V-type mixer (blender), a ribbon mixer (ribbon blender), and a double cone mixer (バブルコーンブレンダー), a mixer such as a Henschel mixer (Henschel mixer) and a concrete mixer, a ball mill, a chopper mill (chopper mill), and the like. When the hydrotalcite is pulverized by a ball mill or the like, the above-mentioned higher fatty acid, alkylsilane, or silane coupling agent may be added to perform surface treatment. The amount of the surface-treating agent to be used may vary depending on the kind of hydrotalcite or the kind of the surface-treating agent, but is preferably 1 to 10 parts by mass based on 100 parts by mass of the hydrotalcite without surface treatment. In the present invention, the surface-treated semi-calcined hydrotalcite is included in the concept of "semi-calcined hydrotalcite" in the present invention.
From the viewpoint of exhibiting the sealing performance of the resin composition of the present invention, the content of the semi-calcined hydrotalcite in the resin composition of the present invention is more than 45% by mass relative to 100% by mass of the nonvolatile component of the resin composition. The content is preferably 50% by mass or more, more preferably 55% by mass or more, and further more preferably 60% by mass or more. The upper limit of the content is not particularly limited as long as the effects of the present invention are exhibited, but the content is preferably 80% by mass or less, more preferably 75% by mass or less, and still more preferably 70% by mass or less, from the viewpoint of transparency of the resin composition and the like.
The resin composition of the present invention may contain a filler other than the semi-calcined hydrotalcite within a range not to impair the effects of the present invention. Examples of the filler other than the semi-calcined hydrotalcite include inorganic fillers such as silica, alumina, barium sulfate, aluminum hydroxide, magnesium hydroxide, calcium carbonate, magnesium carbonate, boron nitride, aluminum borate, barium titanate, strontium titanate, calcium titanate, magnesium titanate, bismuth titanate, titanium oxide, zirconium oxide, barium zirconate, calcium zirconate, and silicate, and organic fillers such as rubber particles, silicone powder, nylon powder, and fluororesin powder. The content of the filler other than the semi-calcined hydrotalcite is preferably 50 parts by mass or less, more preferably 30 parts by mass or less, further preferably 20 parts by mass or less, and still further preferably 10 parts by mass or less, relative to 100 parts by mass of the semi-calcined hydrotalcite.
< Adhesivity-imparting agent >
The resin composition of the present invention may further contain an adhesion-imparting agent. The adhesion-imparting agent is also called a thickener, and is a component for imparting adhesion to the composition. The adhesiveness-imparting agent is not particularly limited, and a terpene resin, a modified terpene resin (hydrogenated terpene resin, terpene-phenol copolymer resin, aromatic modified terpene resin, etc.), coumarone resin, indene resin, or a petroleum resin (aliphatic petroleum resin, hydrogenated alicyclic petroleum resin, aromatic petroleum resin, aliphatic-aromatic copolymer petroleum resin, alicyclic petroleum resin, dicyclopentadiene petroleum resin, hydrogenated product thereof, etc.) is preferably used.
Examples of commercially available products that can be used as the adhesiveness imparting agent include the following. Examples of the terpene RESIN include YS RESIN PX and YS RESIN PXN (both of Yasuhara Chemical Co., Ltd.); examples of the aromatic modified terpene RESIN include YS RESIN TO and TR series (both of which are products of Yasuhara Chemical Co., Ltd.); examples of the hydrogenated terpene resin include CLEARON (クリアロン) P, CLEARON M, CLEARON K series (all of Yasuhara Chemical Co., Ltd.), and the like; examples of the terpene-phenol copolymer resin include YS POLYSTER 2000, POLYSTER U, POLYSTER T, POLYSTER S, マイティエース G (all manufactured by Yasuhara Chemical Co., Ltd.), and the like; examples of the hydrogenated alicyclic petroleum resin include Escorez 5300 series and 5600 series (both manufactured by Exxon Mobil Co., Ltd.); examples of the aromatic petroleum resin include ENDEX 155 (manufactured by Istman chemical Co., Ltd.); examples of the aliphatic aromatic copolymer petroleum resin include Quintone D100 (manufactured by japan regon corporation); examples of the alicyclic petroleum resin include Quintone 1325 and Quintone 1345 (both manufactured by japan regen corporation); examples of the saturated hydrocarbon resin include ARKON P100, ARKON P125, ARKON P140, and TFS 13-030 (all manufactured by Mitsukawa chemical Co., Ltd.).
The softening point of the adhesion-imparting agent is preferably 50 to 200 ℃, more preferably 90 to 180 ℃, and still more preferably 100 to 150 ℃ from the viewpoint of softening the sheet in the laminating step of the resin composition sheet and providing the sheet with desired heat resistance. The softening point was measured by the ring and ball method in accordance with JIS K2207.
The number of the adhesion-imparting agents may be 1 or 2 or more. The content of the tackiness-imparting agent in the resin composition is not particularly limited. However, in the case of using the adhesion-imparting agent, the content thereof is preferably 50% by mass or less, more preferably 40% by mass or less, and still more preferably 30% by mass or less, based on 100% by mass of the nonvolatile component of the resin composition, from the viewpoint of maintaining good sealing performance of the resin composition. On the other hand, in the case of using the adhesion-imparting agent, the content thereof is preferably 5% by mass or more, more preferably 10% by mass or more, based on 100% by mass of the nonvolatile component of the resin composition, from the viewpoint of having sufficient adhesiveness.
From the viewpoint of the adhesiveness, sealing property, transparency and the like of the resin composition, a petroleum resin is preferred. Examples of the petroleum resin include aliphatic petroleum resins, aromatic petroleum resins, aliphatic aromatic copolymerized petroleum resins, and alicyclic petroleum resins. From the viewpoint of the adhesiveness, sealing property, compatibility and the like of the resin composition, aromatic petroleum resins, aliphatic aromatic copolymer petroleum resins and alicyclic petroleum resins are more preferable. In addition, from the viewpoint of improving transparency, an alicyclic petroleum resin is particularly preferable. As the alicyclic petroleum resin, a resin obtained by hydrogenating an aromatic petroleum resin can be used. In this case, the hydrogenation ratio of the alicyclic petroleum resin is preferably 30 to 99%, more preferably 40 to 97%, and further more preferably 50 to 90%. If the hydrogenation ratio is too low, the transparency tends to be lowered by coloring; if the hydrogenation rate is too high, the production cost tends to increase. The hydrogenation rate being determined by the hydrogen of the aromatic ring before and after hydrogenation1The ratio of the peak intensities in H-NMR. The alicyclic petroleum resin is particularly preferably a hydrogenated petroleum resin containing a cyclohexane ring or a dicyclopentadiene hydrogenated petroleum resin. The petroleum resin may be used in 1 kind or in combination of 2 or more kinds. The number average molecular weight Mn of the petroleum resin is preferably 100 to 2000, more preferably 700 to 1500, further preferably 500 to 1000.
< curing agent and/or curing accelerator >
The resin composition of the present invention may contain a curing agent and/or a curing accelerator (preferably a curing accelerator). The curing agent and the curing accelerator may be used alone in 1 kind or in combination of 2 or more kinds. Examples of the curing agent include imidazole compounds, tertiary amine/quaternary ammonium compounds, dimethyl urea compounds, organic phosphine compounds, primary amine/secondary amine compounds, and the like. Examples of the curing accelerator include imidazole compounds, tertiary amine/quaternary ammonium compounds, dimethyl urea compounds, and organic phosphine compounds.
Examples of the imidazole compound as the curing agent and/or the curing accelerator in the present invention include: 1H-imidazole, 2-methylimidazole, 2-phenyl-4-methylimidazole, 2-ethyl-4-methylimidazole, 1-cyanoethyl-2-ethyl-4-methylimidazole, 2-undecylimidazole, 1-cyanoethyl-2-undecylimidazolium trimellitate, 2, 4-diamino-6- (2 '-undecylimidazolyl- (1')) -ethyl-s-triazine, 2-phenyl-4, 5-bis (hydroxymethyl) imidazole, 1-benzyl-2-methylimidazole, 1-benzyl-2-phenylimidazole, 2-methyl-2-methylimidazole, 1-cyanoethyl-2-undecylimidazolium chloride, 2-methyl-2-methylimidazole, 1-methyl-2-phenylimidazole, 2-methylimidazole, 2-phenylimidazole, and (phenylimidazole), 2-dodecyl imidazole, 2-heptadecyl imidazole, 1, 2-dimethyl imidazole, 2-phenyl-4-methyl-5-hydroxymethyl imidazole, 2, 4-diamino-6- (2 '-methylimidazolyl- (1') -ethyl-s-triazine, 2, 4-diamino-6- (2 '-methylimidazolyl- (1')) -ethyl-s-triazine isocyanuric acid adduct, etc. As specific examples of imidazole compounds, examples thereof include Curezol 2MZ, 2P4MZ, 2E4MZ, 2E4MZ-CN, C11Z, C11Z-CN, C11Z-CNS, C11Z-A, 2PHZ, 1B2MZ, 1B2PZ, 2PZ, C17Z, 1.2DMZ, 2P4MHZ-PW, 2MZ-A and 2MA-OK (all manufactured by Kagaku Kogyo Co., Ltd.).
The tertiary amine/quaternary ammonium compound as the curing agent and/or the curing accelerator in the present invention is not particularly limited, and examples thereof include: quaternary ammonium salts such as tetramethylammonium bromide and tetrabutylammonium bromide; diazabicyclo compounds such as DBU (1, 8-diazabicyclo [5.4.0] undecene-7), DBN (1, 5-diazabicyclo [4.3.0] nonene-5), DBU-phenoxide, DBU-octoate, DBU-p-toluenesulfonate, DBU-formate, and DBU-novolak resin (phenoi novolac resin) salt; tertiary amines such as benzyldimethylamine, 2- (dimethylaminomethyl) phenol, and 2,4, 6-tris (dimethylaminomethyl) phenol (TAP), and salts thereof, and dimethylurea compounds such as aromatic dimethylurea and aliphatic dimethylurea.
Examples of the primary/secondary amine-based compound as the curing agent in the present invention include: examples of the aliphatic amines include diethylenetriamine, triethylenetetramine, tetraethylenepentamine, trimethylhexamethylenediamine, 2-methylpentamethylenediamine, 1, 3-bisaminomethylcyclohexane, dipropylenediamine, diethylaminopropylamine, bis (4-aminocyclohexyl) methane, norbornenediamine, and 1, 2-diaminocyclohexane, examples of the alicyclic amines include N-aminoethylpiperazine and 1, 4-bis (3-aminopropyl) piperazine, and examples of the aromatic amines include diaminodiphenylmethane, m-phenylenediamine, m-xylylenediamine, m-phenylenediamine, diaminodiphenylmethane, diaminodiphenylsulfone, and diethyltoluenediamine. Specific examples of the primary/secondary amine-based compound include KAYAHARDA-A (4, 4 '-diamino-3, 3' -dimethyldiphenylmethane, manufactured by Nippon chemical Co., Ltd.).
Specific examples of the dimethylurea compound as the curing agent and/or the curing accelerator in the present invention include: and aromatic dimethylureas such as DCMU (3- (3, 4-dichlorophenyl) -1, 1-dimethylurea), U-CAT3512T (manufactured by San-Apro Co., Ltd.), and aliphatic dimethylureas such as U-CAT3503N (manufactured by San-Apro Co., Ltd.). Among them, aromatic dimethylurea is preferably used from the viewpoint of curability.
Examples of the organophosphinic compound as the curing agent and/or the curing accelerator in the present invention include: triphenylphosphine, tetraphenylphosphonium tetra-p-tolylborate, tetraphenylphosphonium tetraphenylborate, tri-tert-butylphosphonium tetraphenylborate, (4-methylphenyl) triphenylphosphonium thiocyanate, tetraphenylphosphonium thiocyanate, butyltriphenylphosphonium thiocyanate, triphenylphosphine triphenylborane, and the like. Specific examples of the organophosphinic compound include TPP, TPP-MK, TPP-K, TTBuP-K, TPP-SCN, and TPP-S (manufactured by Beixinghua chemical Co., Ltd.).
The total content of the curing agent and the curing accelerator in the resin composition is not particularly limited, but is preferably 5% by mass or less, more preferably 1% by mass or less, based on 100% by mass of the nonvolatile component of the resin composition, from the viewpoint of preventing deterioration in transparency and the like of the sealant layer (resin composition layer). On the other hand, from the viewpoint of suppressing the tackiness of the sealant layer, the total content is preferably 0.0005 mass% or more, more preferably 0.001 mass% or more, based on 100 mass% of the nonvolatile component of the resin composition.
The content of the curing accelerator in the resin composition is not particularly limited, but is preferably 5% by mass or less, more preferably 1% by mass or less, based on 100% by mass of the nonvolatile component of the resin composition, from the viewpoint of preventing deterioration in transparency and the like of the sealant layer (resin composition layer). On the other hand, from the viewpoint of suppressing the tackiness of the sealant layer, the content is preferably 0.0005 mass% or more, more preferably 0.001 mass% or more, based on 100 mass% of the nonvolatile component of the resin composition.
< plasticizer >
The resin composition of the present invention may further comprise a plasticizer. By using the plasticizer, flexibility and moldability of the resin composition can be improved. The plasticizer is not particularly limited, but is preferably a material that is liquid at room temperature. Specific examples of the plasticizer include: and mineral oils such as paraffin-based process oil, naphthenic-based process oil, liquid paraffin, polyethylene wax, polypropylene wax, and vaseline, vegetable oils such as castor oil, cottonseed oil, rapeseed oil, soybean oil, palm oil, coconut oil, and olive oil, and liquid polyalphaolefins such as liquid polybutene, hydrogenated liquid polybutene, liquid polybutadiene, and hydrogenated liquid polybutadiene. As the plasticizer used in the present invention, liquid polyalphaolefins are preferable, and liquid polybutadiene is particularly preferable. Further, the liquid polyalphaolefin is preferably a liquid polyalphaolefin having a low molecular weight from the viewpoint of adhesiveness, and is preferably one having a weight average molecular weight in the range of 500 to 5000, more preferably 1000 to 3000. These plasticizers may be used alone in 1 kind, or in combination of 2 or more kinds. Here, "liquid" means a state of the plasticizer at room temperature (25 ℃ C.). When the plasticizer is used, the content thereof is preferably 50% by mass or less with respect to 100% by mass of the nonvolatile component of the resin composition, from the viewpoint of not adversely affecting electronic devices.
< other ingredients >
The resin composition of the present invention may optionally contain components other than the above-mentioned components to the extent that the effects of the present invention are not impaired. Examples of such components include resins other than the above-mentioned polyolefin resins (for example, epoxy resins, polyurethane resins, acrylic resins, polyamide resins, etc.), thickeners such as Orben and Benton, defoaming agents or leveling agents of silicone type, fluorine type and polymer type, and adhesion imparting agents such as triazole compounds, thiazole compounds, triazine compounds and porphyrin compounds.
< method for producing resin composition >
The method for producing the resin composition of the present invention is not particularly limited as long as the water content can be sufficiently reduced. For example, the resin composition having a reduced water content can be produced by mixing the respective components with a solvent used as needed and drying the obtained compound.
The drying of the mixture is carried out more conveniently by heating. The heating may be carried out under normal pressure or under reduced pressure. The heating temperature and heating time may vary depending on the components used. The heating temperature and heating time for sufficiently reducing the water content can be appropriately set by those skilled in the art according to the components to be used.
< resin sheet and method for producing same >
The present invention also provides a resin sheet comprising a support and a layer of the resin composition of the present invention (hereinafter also simply referred to as "resin composition layer") provided on the support.
The resin composition layer of the resin sheet may be formed by a method known to those skilled in the art. For example, the coating composition can be formed by preparing a varnish in which the above components are dissolved in an organic solvent, applying the varnish to a support, and drying the applied varnish. The nonvolatile component of the varnish is preferably 20 to 80% by mass, more preferably 30 to 70% by mass.
Examples of the organic solvent include: ketones such as acetone, Methyl Ethyl Ketone (MEK) and cyclohexanone; acetates such as ethyl acetate, butyl acetate, cellosolve acetate, propylene glycol monomethyl ether acetate, carbitol acetate, etc.; cellosolves such as cellosolve, carbitols such as butyl carbitol; aromatic hydrocarbons such as toluene and xylene; dimethylformamide, dimethylacetamide, N-methylpyrrolidone, and the like. The organic solvent may be used alone in 1 kind, or 2 or more kinds may be used in combination.
Drying of the varnish is carried out simply by heating. The heating may be carried out under normal pressure or under reduced pressure. The heating temperature and heating time may vary depending on the components and organic solvent used. The heating temperature and heating time for sufficiently reducing the water content can be appropriately set by those skilled in the art according to the components and the organic solvent to be used. The preferable conditions for adjusting the water content of the resin composition layer to 2500ppm or less are as described above.
When a resin sheet is produced using a resin composition containing a polyolefin-based resin having an acid anhydride group and a polyolefin-based resin having an epoxy group, the acid anhydride group and the epoxy group are reacted to form a crosslinked structure in advance, whereby the moisture permeability resistance of the layer of the resin composition is improved, and a resin sheet having higher sealing performance (barrier performance against moisture and oxygen in the air, etc.) can be obtained.
The thickness of the resin composition layer in the resin sheet is preferably 1 to 1000. mu.m, more preferably 2 to 800. mu.m.
Examples of the support for the resin sheet include: polyolefins such as polyethylene, polypropylene, and polyvinyl chloride, cycloolefin polymers, polyesters such as polyethylene terephthalate (hereinafter sometimes referred to simply as "PET") and polyethylene naphthalate, and plastic films such as polycarbonate and polyimide. The surface of the support to be bonded to the resin composition layer may be subjected to a mold release treatment. Examples of the release treatment include release treatment using a release agent such as a silicone resin-based release agent, an alkyd resin-based release agent, or a fluororesin-based release agent.
The thickness of the support is not particularly limited, but is preferably 10 to 150 μm, more preferably 20 to 100 μm, from the viewpoint of handling of the resin sheet.
As the support for the resin sheet, a support having a barrier layer (for example, a plastic film having a barrier layer) is preferable. Examples of the barrier layer include inorganic films such as a silicon dioxide vapor deposited film, a silicon nitride film, and a silicon oxide film. The barrier layer may be formed of a plurality of inorganic films (e.g., a silicon dioxide vapor deposited film). The barrier layer may be composed of an organic material and an inorganic material, or may be a composite multilayer of an organic layer and an inorganic film.
As the support having a barrier layer, for example, a support having a Water Vapor Transmission Rate (WVTR) of 0.0005 (g/m)2/24hr) or less. Examples of the high-barrier plastic film include materials obtained by laminating an inorganic film such as silicon oxide (silicon dioxide), aluminum oxide, magnesium oxide, silicon nitride, silicon oxynitride, SiCN, or amorphous silicon in a single layer or a plurality of layers on the surface of a plastic film by a chemical vapor deposition method (for example, a chemical vapor deposition method using heat, plasma, ultraviolet light, vacuum heat, vacuum plasma, or vacuum ultraviolet light) or a physical vapor deposition method (for example, a vacuum deposition method, a sputtering method, an ion plating method, a laser deposition method, or a molecular beam epitaxy method) (for example, see japanese patent laid-open publication No. 2016 185185705, japanese patent No. 5719106, japanese patent No. 5712509, and japanese patent No. 5292358). In order to prevent the inorganic film from cracking, it is preferable to alternately laminate the inorganic film and a transparent planarizing layer (e.g., a transparent plastic layer).
Further, as the support having the barrier layer, for example, a support having a WVTR of 0.01 (g/m)2/24hr) of 1 (g/m) or more2/24hr) or less. Examples of the medium-barrier plastic film include those produced by the following method: examples of the barrier layer include a method of depositing an inorganic film containing an inorganic substance such as silicon oxide (silicon dioxide), aluminum oxide, magnesium oxide, silicon nitride, silicon oxynitride, SiCN, or amorphous silicon on the surface of a substrate, and a method of applying a coating liquid containing a metal oxide and an organic resin having a barrier property to a substrate and drying the coating liquid (see, for example, japanese patent laid-open nos. 2013 and 108103 and 4028353).
The water vapor transmission rate can be measured as follows. First, test pieces of 60mm phi were prepared by punching a plastic film having a barrier layer. According to JIS Z0208: 1976 and has a transmission area of 2.826 × 10-3m27.5g of calcium chloride was weighed in a moisture permeable cup made of aluminum (60 mm. phi.), and a test piece was mounted in the moisture permeable cup. Calcium chloride was added, and the initial mass of the moisture-permeable cup equipped with the test piece was measured with a precision balance. Next, the moisture permeable cup was left to stand in a constant temperature laboratory at 40 ℃ and 90% RH for 24 hours, calcium chloride was added, and the mass of the moisture permeable cup with the test piece attached thereto after moisture permeation was measured with a precision balance. The mass increment (mass after moisture permeation-initial mass) was defined as the water vapor transmission rate, and the water vapor transmission rate (g/m) was calculated from the water vapor transmission rate, the transmission area and the standing time2/24hr)。
As the support having the barrier layer, commercially available products can be used. Examples of commercially available products of the intermediate barrier plastic film include "KURARISTER CI" manufactured by Coli, TECHBARRIER HX "," TECHNBARRIER LX "and TECHNBARRIER L" manufactured by Mitsubishi resin corporation, "IB-PET-PXB" manufactured by Dainippon printing corporation, and "GL, GX series" manufactured by letterpress printing corporation; examples of commercially available products of high-BARRIER plastic films include "X-BARRIER" manufactured by Mitsubishi resin corporation.
The resin composition layer provided on the support is preferably protected in advance with a protective film. The lamination of the protective film on the resin composition layer can be performed using a known apparatus. Examples of the equipment used for laminating the protective film include a roll laminator, a press laminator, and a vacuum press laminator.
Examples of the protective film include the above-mentioned plastic films. The surface of the protective film to be bonded to the resin composition layer is preferably subjected to a mold release treatment. Examples of the release treatment include release treatment using a release agent such as a silicone resin-based release agent, an alkyd resin-based release agent, or a fluororesin-based release agent.
The thickness of the protective film is not particularly limited, but is preferably 10 to 150 μm, more preferably 20 to 100 μm, from the viewpoint of handling properties of the resin sheet.
In order to suppress the absorption of moisture by the resin composition layer after drying, it is preferable to use a protective film having a barrier layer. Examples of the protective film having a barrier layer include the above-described plastic films having a barrier layer. From the viewpoint of cost and the like, the plastic film having a barrier layer used for the protective film is preferably a medium barrier plastic film as described above.
< use >)
The resin composition and the resin sheet of the present invention can be used for sealing electronic devices. The electronic device is preferably an electronic device having low resistance to moisture, such as an organic EL device or a solar cell. That is, the resin composition and the resin sheet of the present invention can be suitably used for sealing an electronic device having low moisture resistance, such as an organic EL device and a solar cell.
Examples
The present invention will be described in more detail with reference to the following examples, but the present invention is not limited to the following examples, and can be carried out with appropriate modifications within the scope that can meet the gist of the context, and these are included in the technical scope of the present invention. Unless otherwise specified, "part" and "%" in the amounts of the components and the amount of the copolymerized units mean "part by mass" and "% by mass", respectively.
< ingredient >
The ingredients used in the examples and comparative examples are shown below;
(polyolefin resin)
"HV-1900" (manufactured by JXTG energy Co., Ltd.): polybutene, number average molecular weight 2900
"HV-300M" (manufactured by Toho chemical industry Co., Ltd.): maleic anhydride modified liquid polybutene with anhydride group concentration of 0.77mmol/g and number average molecular weight of 2100
"T-YP 341" (manufactured by Astro PMC Co., Ltd.): glycidyl methacrylate modified propylene-butene random copolymer having propylene unit/butene unit 71%/29%, epoxy group concentration of 0.638mmol/g, number average molecular weight of 155000
(semi-calcined hydrotalcite)
"DHT-4C" (manufactured by Kyowa chemical industries Co., Ltd.): semi-calcined hydrotalcite with average particle size of 400nm and BET specific surface area of 15m2/g
(Adhesivity-imparting agent)
"ARKON P125" (manufactured by Mitsukawa chemical Co., Ltd.): saturated hydrocarbon resin containing cyclohexane ring, softening point 125 deg.C
(curing accelerators)
2,4, 6-tris (dimethylaminomethyl) phenol (hereinafter abbreviated as "TAP") (Kayaksu Akzo, Kayaku Akzo Co., Ltd.): a curing accelerator.
< example 1 >
Varnishes having the compositions shown in the following tables were prepared in accordance with the following procedures, and the obtained varnishes were used to prepare resin sheets. The amount (parts) of each component used in the following table indicates the amount of nonvolatile components in the varnish. The following table shows the content of the semi-calcined hydrotalcite used as the semi-calcined hydrotalcite per 100 mass% of the nonvolatile components in the resin composition.
Specifically, maleic anhydride-modified liquid polybutene (HV-300M, manufactured by Toho chemical industries Co., Ltd.), polybutene (HV-1900, manufactured by JXTG energy Co., Ltd.), and half-calcined hydrotalcite (DHT-4C, manufactured by Kyowa chemical industries Co., Ltd.) were dispersed in a Swasol (スワゾール) solution (nonvolatile matter 60%) of a saturated hydrocarbon resin having a cyclohexane ring (an adhesion imparting agent, ARKON P125, manufactured by Mikan chemical Co., Ltd.) to obtain a mixture. To the obtained mixture, a Swasol solution (nonvolatile content: 20%) of a glycidyl methacrylate-modified propylene-butene random copolymer (T-YP341, manufactured by seiko PMC), a curing accelerator (TAP, manufactured by akkusu corporation) and toluene were added, and the obtained mixture was uniformly dispersed by a high-speed rotary mixer to obtain a varnish of a resin composition. The resulting varnish was uniformly applied to a release-treated surface of a polyethylene terephthalate (PET) film "SP 4020" (PET: 50 μm, manufactured by TOYO CLOTH Co., Ltd.) treated with a silicone-based release agent by means of a die coater, heated at 130 ℃ for 30 minutes and then at 160 ℃ for 30 minutes, to obtain a resin sheet having a resin composition layer with a thickness of 25 μm.
< example 2 >
A varnish of a resin composition and a resin sheet having a resin composition layer with a thickness of 25 μm were produced in the same manner as in example 1, except that the amount of the semi-calcined hydrotalcite (DHT-4C, manufactured by Kyowa chemical Co., Ltd.) was changed from 300 parts to 250 parts.
< example 3 >
A varnish of a resin composition and a resin sheet having a resin composition layer with a thickness of 25 μm were produced in the same manner as in example 1, except that the amount of the semi-calcined hydrotalcite (DHT-4C, manufactured by Kyowa chemical Co., Ltd.) was changed from 300 parts to 200 parts.
< example 4 >
A varnish of a resin composition and a resin sheet having a resin composition layer with a thickness of 25 μm were produced in the same manner as in example 1, except that the amount of the semi-calcined hydrotalcite (DHT-4C, manufactured by Kyowa chemical Co., Ltd.) was changed from 300 parts to 100 parts.
< comparative example 1 >
Varnishes having the compositions shown in the following tables were prepared in accordance with the following procedures, and the obtained varnishes were used to prepare resin sheets. The amount (parts) of each component used in the following table indicates the amount of nonvolatile components in the varnish. The content of the semi-calcined hydrotalcite per 100 mass% of the nonvolatile components of the resin composition is shown in the following table.
Specifically, maleic anhydride-modified liquid polybutene (HV-300M, manufactured by Toho chemical industries Co., Ltd.), polybutene (HV-1900, manufactured by JXTG energy Co., Ltd.), and half-calcined hydrotalcite (DHT-4C, manufactured by Kyowa chemical industries Co., Ltd.) were dispersed in a Swasol solution (nonvolatile matter 60%) of a saturated hydrocarbon resin having a cyclohexane ring (an adhesion imparting agent, ARKON P125, manufactured by Mikan chemical Co., Ltd.) by a three-roll mill to obtain a mixture. To the obtained mixture, a Swasol solution (nonvolatile content: 20%) of a glycidyl methacrylate-modified propylene-butene random copolymer (T-YP341, manufactured by seiko PMC), a curing accelerator (TAP, manufactured by akkusu corporation) and toluene were added, and the obtained mixture was uniformly dispersed by a high-speed rotary mixer to obtain a varnish of a resin composition. The varnish thus obtained was uniformly applied to a release-treated surface of a PET film "SP 4020" (PET: 50 μm, manufactured by TOYO CLOTH Co., Ltd.) treated with a silicone-based release agent by means of a die coater, and the resultant was heated at 130 ℃ for 30 minutes and then at 160 ℃ for 15 minutes to obtain a resin sheet having a resin composition layer with a thickness of 25 μm.
< comparative example 2 >
A varnish of a resin composition was prepared in the same manner as in example 1, and the obtained varnish was uniformly applied to a release-treated surface of a PET film "SP 4020" (PET: 50 μm, TOYO CLOTH Co., Ltd.) treated with a silicone-based release agent by means of a die coater and heated at 130 ℃ for 30 minutes to obtain a resin sheet having a resin composition layer with a thickness of 25 μm.
< comparative example 3 >
A varnish of a resin composition was prepared in the same manner as in example 4, and the obtained varnish was uniformly applied to a release-treated surface of a PET film "SP 4020" (PET: 50 μm, TOYO CLOTH Co., Ltd.) treated with a silicone-based release agent by means of a die coater and heated at 130 ℃ for 60 minutes to obtain a resin sheet having a resin composition layer with a thickness of 25 μm.
< comparative example 4 >
A resin sheet having a resin composition layer with a thickness of 25 μm was produced in the same manner as in comparative example 3, except that the varnish having the formulation of comparative example 4 shown in Table 1 below was prepared.
The resin composition layers of the respective resin sheets obtained in examples and comparative examples were evaluated for transparency by total light transmittance, moisture permeation resistance (sealing performance) by average molecular permeation distance, and suppression of deterioration of a sealing target portion by internal moisture (sealing performance) by reflectance ratio.
< Water content of resin composition layer >
The resin sheets prepared in examples and comparative examples were cut into a length of 70mm and a width of 40mm, and the support (i.e., the PET film "SP 4020" treated with a silicone-based release agent) was peeled off, and the resin composition layer was folded and placed in a sufficiently dried screw vial (screen visual container) (VABH17, manufactured by mitsubishi chemical analysis co., ltd.) and placed in an electric furnace (VA-236S, manufactured by mitsubishi chemical analysis co., ltd.) directly connected to a Karl Fischer (Karl Fischer) tester (CA-310, manufactured by mitsubishi chemical analysis co., ltd.). In N2In the gas flow, the temperature of the electric furnace was raised to 250 ℃, and the water desorbed from the measurement sample was captured in the karl fischer measurement solution, and the mass of the water was measured by a conventional method. According to the measured mass of water, to the resin groupThe water content (ppm) of the resin composition layer was calculated based on the mass of the entire compound. The results are shown in the following table.
< Total light transmittance >
The resin sheets prepared in examples and comparative examples were cut into a length of 50mm and a width of 20mm, and the cut resin sheets were laminated on a glass plate (a microscope slide glass having a length of 76mm, a width of 26mm and a thickness of 1.2mm, a white glass slide glass S1112 edging No. 2 manufactured by Sonlanga Nitz industries, Ltd.) by a batch type vacuum laminator (V-160 manufactured by Nichigo-Morton Co., Ltd.) in such a manner that the resin composition layer was in contact with the glass plate. The lamination conditions were 80 ℃ and 30 seconds after the decompression time, and the pressure was applied at 0.3MPa for 30 seconds. Then, the PET film of the resin sheet was peeled off, and the light transmittance spectrum of the exposed resin composition layer was measured by an optical fiber spectrophotometer (MCPD-7700, model 311C, manufactured by Otsuka Denshi Co., Ltd., external light source unit: halogen lamp MC-2564(24V, 150W standard)) equipped with a phi 60mm integrating sphere (model SRS-99-010, reflectance 99%), to calculate the total light transmittance (%) at a wavelength of 450nm, and evaluated in accordance with the following criteria. The results are shown in the following table. The distance between the integrating sphere and the sample (laminate) was set to 0mm, and glass was used as a reference;
good (∘): total light transmittance of 90% or more
Poor (x): the total light transmission is less than 90%.
< average moisture intrusion distance >
Alkali-free glass having a side length of 50mm × 50mm was washed with boiled isopropyl alcohol for 5 minutes and dried at 150 ℃ for 30 minutes or more. Next, UV ozone cleaning of the alkali-free glass was performed. A calcium film (purity 99.8%) (thickness 200nm) was deposited on the alkali-free glass after cleaning using a mask whose distance from the end was set to 2 mm.
Resin sheets having a laminated structure of a PET/aluminum foil/resin composition layer having the same resin composition layer as in examples and comparative examples were obtained in the same manner as in examples and comparative examples except that an aluminum foil/PET composite film "AL 1N30 with PET" (aluminum foil: 30 μm, PET: 25 μm, manufactured by toyoyo aluminum vending corporation, east sea) was used as the support.
The alkali-free glass vapor-deposited with the calcium film was bonded to a resin sheet in a glove box by a thermal laminator (manufactured by Fuji-Pulley Co., Ltd., Lamipar DAiSY A4(LPD2325)) so that the calcium film was in contact with the resin composition layer, to obtain a sample for evaluation.
If calcium comes into contact with water to form calcium oxide, it becomes transparent. Therefore, the intrusion of moisture into the sample for evaluation can be evaluated by measuring the distance (mm) from the end of the sample for evaluation to the calcium film.
The distance from the end of the sample for evaluation obtained above to the calcium film was measured at 8 places by a Measuring Microscope (Measuring Microscope) MF-U manufactured by Sanfeng corporation, and the average value thereof was X2.
Subsequently, the sample for evaluation was put into a constant temperature and humidity chamber set at a temperature of 85 ℃ and a relative humidity of 85% RH. The distance from the end of the sample for evaluation to the calcium film after being charged into the constant temperature and humidity cell for 40 hours was measured at 8 points, and the average value thereof was X1 (mm).
From the obtained X1 and X2, the average moisture penetration distance X (X1 to X2) into the calcium film after being charged into the constant-temperature and constant-humidity cell was calculated, and the moisture permeability resistance of the resin composition layer under high-temperature and high-humidity conditions was evaluated according to the following criteria. The higher the moisture permeation resistance, the slower the moisture invasion rate can be, and the smaller the value of the average moisture invasion distance X. The results are shown in the following table. In the following table, when X is less than 0.1mm, it is indicated as "< 0.1". Further, with respect to comparative examples 3 and 4 (in which X1 could not be measured due to deterioration of the calcium membrane due to moisture), the result was evaluated as poor (X);
good (∘): x is less than 1mm
Poor (x): x is 1mm or more, or X1 could not be measured due to deterioration of the calcium film by moisture.
< reflectance ratio >
Alkali-free glass having a side length of 50mm × 50mm was washed with boiled isopropyl alcohol for 5 minutes and dried at 150 ℃ for 30 minutes or more. Next, UV ozone cleaning of the alkali-free glass was performed. A calcium film (purity 99.8%) (thickness 200nm) was deposited on the alkali-free glass after cleaning using a mask whose distance from the end was set to 2 mm.
Resin sheets having a laminated structure of a PET/aluminum foil/resin composition layer having the same resin composition layer as in examples and comparative examples were obtained in the same manner as in examples and comparative examples except that an aluminum foil/PET composite film "AL 1N30 with PET" (aluminum foil: 30 μm, PET: 25 μm, manufactured by toyoyo aluminum vending corporation, east sea) was used as the support.
The alkali-free glass vapor-deposited with the calcium film was bonded to a resin sheet in a glove box by a thermal laminator (manufactured by Fuji-Pulley Co., Ltd., Lamipar DAiSY A4(LPD2325)) so that the calcium film was in contact with the resin composition layer, to obtain a sample for evaluation.
The reflectance spectrum of the thus-obtained sample for evaluation was measured with a fiber-optic spectrophotometer (MCPD-7700, model 311C, manufactured by Otsuka Denshi Co., Ltd., external light source unit: halogen lamp MC-2564(24V, 150W standard)) equipped with an integrating sphere (model SRS-99-010, reflectance 99%) having a diameter of 60mm, and the reflectance (%) at a wavelength of 850nm was calculated and designated as Y2.
Next, the sample for evaluation was heated in a glove box with a hot plate at a temperature of 80 ℃ for 39 hours, and then the reflectance spectrum of the heated sample for evaluation was measured, and the value was defined as Y1.
The reflectance ratio Y (Y1/Y2) was calculated from the obtained Y1 and Y2, and the suppression of the deterioration of the calcium film due to the moisture contained in the semi-calcined hydrotalcite in the resin composition layer was evaluated according to the following criteria. The results are shown in the following table. At this time, in comparative examples 1 to 4 (in which reflectance spectrum Y1 could not be measured due to deterioration of the calcium film by moisture), the result was evaluated as poor (x);
good (∘): the reflectance ratio Y is 0.90 or more
Eligibility (Δ): the reflectance ratio Y is less than 0.90
Poor (x): the reflectance spectrum Y1 could not be measured due to the deterioration of the calcium film by moisture.
[ Table 1]
Possibility of industrial utilization
The resin composition of the present invention and the resin sheet using the same can be used for sealing electronic devices (e.g., organic EL devices, sensor devices, solar cells, etc.).
The present application is based on Japanese patent application No. 2019-180606 filed in Japan, and the contents thereof are all included in the present specification.
Claims (8)
1. A resin composition comprising a polyolefin-based resin and a semi-calcined hydrotalcite,
the content of the semi-calcined hydrotalcite exceeds 45% by mass based on 100% by mass of nonvolatile components in the resin composition, and the water content is 2500ppm or less based on the mass of the entire resin composition.
2. The resin composition according to claim 1, wherein the water content is 2000ppm or less on a mass basis relative to the entire resin composition.
3. The resin composition according to claim 1 or 2, wherein the content of the semi-calcined hydrotalcite is more than 45% by mass and 80% by mass or less with respect to 100% by mass of nonvolatile components of the resin composition.
4. The resin composition according to any one of claims 1 to 3, which is used for sealing an electronic device.
5. The resin composition according to claim 4, wherein the electronic device is an organic EL device or a solar cell.
6. A resin sheet having: a support, and a layer of the resin composition according to any one of claims 1 to 3 provided on the support.
7. The resin sheet according to claim 6, which is used for sealing an electronic device.
8. The resin sheet according to claim 7, wherein the electronic device is an organic EL device or a solar cell.
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WO2017057708A1 (en) * | 2015-09-30 | 2017-04-06 | 味の素株式会社 | Resin composition for sealing |
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CN109804035A (en) * | 2016-10-04 | 2019-05-24 | 味之素株式会社 | The resin combination and sealing sheet of sealing |
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CN107409447A (en) * | 2015-03-20 | 2017-11-28 | 味之素株式会社 | The manufacture method of packaging body |
WO2017057708A1 (en) * | 2015-09-30 | 2017-04-06 | 味の素株式会社 | Resin composition for sealing |
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